Textile fabric and method of preparation thereof



Patented Nov. 110, 1942 UNITED TEXTILE FABRIC AND METHOD OF PREPARATION THEREOF William W. Trowell, Greenvllle, 0., assignor to Hercules Powder Company, W

llmington, DeL,

a corporation of Delaware No Drawing. Application July 22, 1939, Serial No. 285,865

16 Claims.

'the resin to an insoluble and infusible form.

It is an object of this invention to provide atextile fabric having an improved permanent, thermoplastic finish which is either soft and flexible, or stiff and starched-like.

Another object of this invention is to provide a method for finishing textile so as to produce on the fabric a permanent, thermoplastic finish which is either soft and flexible, or stifland starched-like.

Other objects of the invention will be obvious from the following description.

The above objects may be accomplished in accordance with this invention by impregnating a textile fabric with an aqueous emulsion of a solution comprising ethyl cellulose and a thermoplastic, alkali-resistant, synthetic resin compatible with ethyl cellulose.

I have found that the use of a resin of the type defined above with ethyl cellulose provides a textile finish which exhibits notable improvements over the finishes obtainable with ethyl cellulose and plasticizer combinations or combinations of ethyl cellulose and curing type resins.

I have found, in accordance with this invention, that rosin modified alkyd resins, such as rosin modified or hydrogenated rosin modified terpene-maleic anhydride resins, rosin-modified maleate resins; drying oil modified terpenemaleic anhydride resins; polymerized hydrocarbon resins, such as polymerized naphthalene,

polymerized coumarone-indene, or hydrogenated forms thereof; 100% phenolic resins; polyhydric alcohol esters of hydrogenated rosin, as well as resins of othertypes which are of a thermoplastic character, arealkali-resistant and are compatible with ethyl cellulose, may be used to provide the desirable features of my invention. Where optimum results are desirable, I prefer to employ resins falling within the above classifica- 'tion which are light in color and which have a content in the range of'about 43% to about 51%, 50 v and preferably from about 44% to about 48%. The viscosity characteristics of the ethyl cellulose used will depend upon the properties desired in the ultimate composition.

The method for treating textile fabrics to provide the features of my invention comprises impregnating a textile fabric with an aqueous emulsion of a solution of ethyl cellulose and a thermoplastic, alkali-resistant synthetic resin compatible with ethyl cellulose, removing excess emulsion from the fabric, evaporating the water and solvent from the fabric and subjecting the fabric to a heating treatment. Preferably, the treated fabric is ironed, by heat and pressure, after removal of excess emulsion and evaporation of water and solvents. :The ironing process may be accomplished by passing the treated fabric over a series of heated rolls, or the fabric may be finished by drying the fabric in a blast of heated air, subsequently passing the treated fabric between heated pressure rolls. The ironing temperature used will. lie within the range of about 180 Fnto about 400 F., and preferably will be within the range of about 240 F. to about 280 F., the actual temperature used being dependent upon the type of fabric employed and the composition deposited on the fabric.

In practicing the process according to my invention, the excess emulsion may be removed 80 conveniently from the fabric by passing the treated fabric between padded squeeze rolls. The amount of emulsion remaining in the fabric will determine to a large extent the final stiffness,

hand and body of the finished fabric. By 1111- pregnating the fabrics with emulsions containing different concentrations of ethyl cellulose and the synthetic resin, it is possible to vary the amount of solids deposited in the fabric and thereby to vary the hand and body of the finished fabric as desired.

- In any event, the amount of emulsion remaining in the fabric, after the excess emulsion has been removed, will be such that the amount of dry, film-forming composition remaining in the fabric will, at the end of my procedure, be insufficient to fill the interstices between threads,

or to form a continuous coating over the surface of the fabric, but will be sufiiclent to provide the finished fabric hereinafter described.

In practicing my invention, I apply my emulsions so as to leave in the fabric an amount of thermoplastic substance in the dry state not over about 40% of the weight of the untreated fabric,

and preferably not over about 20% of the weight of the untreated fabric. The amount of dry thermoplastic substance retained in the fabric is controlled depending on whether a soft, flexible permanent finish on the one hand or a still,

starched-like finish on the other hand, or any finish intermediate thereto, is desired.

The textile fabric produced in accordance with this invention will be characterized by possessing a permanent finish comprising ethyl cellulose and a thermoplastic, alkali-resistant synthetic resin compatible with ethyl cellulose. The tex tile fabric will he further characterized by having a fullness and body which is retained on aging and to a very substantial extent after repeated washings. It will have either a soft handle or a stiff finish depending on the amount of impregnating composition introduced into the fabric. The stiffness or sizing of the fabric will disappear on laundering but will be regenerated on ironing the fabric due to the re-fusing of the ethyl cellulose and resin composition by application of heat and pressure. The fabric will be permanently pliable and pervious to both moisture and air.

The aqueous emulsion of ethyl cellulose and a synthetic resin of the character defined may, if desired, contain a softening or plasticizing agent for further lowering the softening point of the composite material. The plasticizer used will preferably be one which is resistant to alkaline solutions. It will also desirably be compatible with the ethyl cellulose and the ethyl celluloseresin mixture. The plasticizer may be either of the liquid type or the solid type. Solid plasticizers are preferred since they contribute to the fullness and body of the finished fabric more than the liquid plasticizers. Suitable plasticizers are hydrogenated methyl abietate; hydrogenated ethyl abietate; triphenyl phosphate; tricresyl phosphate; tributyl phosphate; methyl phthalyl methyl glycollate; ethyl phthalyl ethyl glycollate; di-(para-tertiary butyl phenyl), mono-(S-tertiary butyl-Z-xenyl) phosphate, etc.

The aqueous emulsions used in accordance with this invention will preferably be prepared by emulsifying a solution of the ethyl cellulose, the synthetic resin, and the plasticizer, if one is used, in a suitable common solvent therefor, preferably a mixed solventcomprising' light aromatic and petroleum hydrocarbons and butanol. Suitable emulsifying agents are, for example, the alkali metal salts of the higher aliphatic half ester sulfates, as sodium lauryl sulfate, sodium stearyl sulfate, etc; sulfonated oils, as sulfonated castor oil, sulfonate'd olive oil, etc.; soaps, as sodium stearate, potassium oleate, sodium oleate, etc; alkali metal salts of alkyl naphthalene sulionic acids, as, sodium butyl naphthalene sulfohate, sodium isopropyl naphthalene sulfonate, etc.

The ratio of resin to ethyl cellulose which I may use in my treating compositions will depend on the particular resin used and on the type of finish desired. The softness or stiffness of the finish will, of course, depend also on the amount of solid composition deposited in the fabric. Generally speaking, the resin will be used in an a still, starched-like finish. Generally speaking, however, a maximum of about 40% by weight of solid, thermoplastic substance in the fabric, basedon the weight of the untreated fabric, is contemplated. For most purposes not over about 20% by weight is contemplated.

The concentration of the solid ingredients of the emulsions used in my invention may be varied over wide ranges merely by diluting the concentrated emulsion with water. By adjusting the water content of the emulsions in this manner, I

am enabled to very effectively control the amount.

of solid thermoplastic substance deposited in the fabric, and thereby to control the stiffness of the finished fabric as desired.

The following examples are illustrative of my invention:

Example I Two hundred parts by weight of solution a were added to 100 parts by weight of solution b and emulsified together by passing through a colloid mill or homogenizing mill.

One part by weight of the emulsion was then diluted with three parts by weight of water. The dilutedemulsion so obtained was used to impregnate 2.85 yard sheeting. The excess emulsion was squeezed from the fabric and the fabric dried amount within the range of about 5% to about 1 80% of the weight of the ethyl cellulose content, and preferably about 25% to about of the weight of the ethyl cellulose.

improved process of finishing is applicable to any of the textile materials such as, for ear-- ample, organdy, lace, broadcloth, cotton, wool,

rayon, etc. Naturally, due to different qualities of fabric to be treated, their weight, their degree of absorbency, etc, it is impossible to define the amount of i a soft, fieitibie finish or suited to provide cit er *egnating composition reseveral hours in the air to evaporate all solvents. The dried fabric was then ironed at a temperature of 310 R, giving a fabric having a stiffness of 69 milligrams as measured on the Gurley stiflness tester.

Example 11 The following solutions were prepared:

Parts by weight (a) Ethyl cellulose 32 Trlphenyl phosphate 6 Glycerol ester of hydrogenated rosin"; 20

Solutions a. and b were emulsified together as in Example I.

One part by weightoi the emulsion was then diluted with three parts by weight of water. The diluted emulsion was used toimpregnat 2.85

yard sheeting as in Example 1. After drying and ironing at a, temperature of 280 F., the finished fabric had a stiffness of 70 milligrams as measured on the Gurley stiffness tester; By ironing the same fabric at a temperature of 310 F. a stiffness of 81 milligrams was obtained.

Example I" The following solutions were prepared:

Parts by weight (a) Ethyl cellulose 32 Triphenyl phosphate 16 Glycerol ester of hydrogenated rosin xylol 106 Hi flash naphtha 20 Butanol 16 Total 200 (b) Potassium oleate 1.5: Water 98.5

Total 100 .Solutions a and b were emulsified together as in Example I. w

One part by weight of the emulsion was then diluted with parts by weight of water. The diluted emulsion was used to impregnate 80 x 80 print cloth, the excess emulsion squeezed from the fabric and the treated fabric dried over cans at a temperature of 250 F. The resulting finished-fabrlc had good body, was quite stiff, and contained about 1 per cent by weight of solids.

The printed colors showed increased brightness and increased sharpnessof detail as compared to the original fabric.

Example IV perature of 250-260" F. The lace curtain, as a.

result of the above treatment, had acquired excellent draping qualities. The fabric does not diminish in stiffness or draping qualities on being draped over windows for extended periods. After laundering and ironing, the original draping qualities are regenerated.

Example V One part by weight of the undiluted emulsion I prepared in Example 111 was diluted with 20 parts by weight of water and the dilute emulsion used to impregnate 136 x 60 carded broadcloth. Excess emulsion was squeezed from the fabric and the treated fabric was dried over a tenter frame at a temperature of about 220 F. The resulting fabric contained about 0.9% solid and had a soft handle and an improved fullness.

Example VI The following solutions were prepared:

Parts by weight (a) Ethyl cellulose 32 Hydrogenated naphthalene polymer, M. P. 130 C.

Triphenyl phosphate 16 Xylol 106 Hi flash naphtha; 20

Butanol the amount of solids impregnated in the fabric I as determined by extraction with a toluol-butanol solvent are shown. Variation of the dilution of the emulsion controls the amount of solids deposited in the fabric and as a consequence, the stiflness of the fabric.

Tests 1 Solids Stiffness 0i Emulsion used deposited of fabric in fabric (Gurlcy) Pe cent 111g. 1. Emulsion of Ex. VI 15. 7 300 2. 1 part emulsion of Ex. VI, 1 part water 0. 4 145 3. 1 part emulsion of Ex. VI, 2 parts water 3. 7 89 4. 1 part emulsion of Ex. VI, 4 parts water.v 3. 6 103 5. 1 part emulsion of Ex. VI. 8 parts water 2. l 75 6. 1 part emulsion of Ex. VI, 15 parts water. 1.2 72 7. 1 art emulsion of Ex. VI, 20 parts water. 0. 97 46 S. ntreated fabric 24 Example VII The following solutions were prepared:

Parts by weight (a) Ethyl cellulose 32 H y d r o g e n a t e d coumarone-indene resin, M. P. 120 C 16 Triphenyl phosphate 10 Xylo] -1 106 Hi flash naphtha 20 Butanol 16 Total 200 (b) Potassium o1eate 1.5 Water 98.5

Total 100 grams as measured on the Gurley stiffnesstester.

Example VIII The following solutions were prepared:

Parts by weight (a)' Ethyl cellulose 32 Glycerol ester of hydrogenated rosin 10 Di- (para-tertiaryb u ty 1 phenyl) mono-(5-tertiary b u t y 1-2 xenyl) phosphate 16 Xylol 106 Hi flash naphtha 20 Butanol 16 4 2,301,480 (b) Potassium oleateru' 1.5 described and claimed is in no way limited Water 98.5 thereby. 1

- I This application forms a. continuation-in-part Total 100 of my application Serial No. 199,042, filed Febru- 5 ary 11, 1938, entitled Textile fabrics and meth- Solutions a and b were in Example VI.

emulsified together as One part by weight of the emulsion was then diluted with three parts by weight of water. The

diluted emulsion was used to impregnate 2.85

yard sheeting by the procedure described in Example VII. The impregnated fabric had every stiff and crispy finish and a stiffness of 140 milligrams as measured on the Gurley stiffness tester.

Solutions a and b were emulsified together as in Example VI.

One part by weight of the emulsion was then diluted with three parts by weight of water. The diluted emulsion was used to impregnate 2.85 yard sheeting by the procedure described in Example VII. The impregnated fabric had a good body and acrisp finish.

The textile fabrics produced in accordance withthe process of thisinvention possess several im-- portant advantages over similar fabrics finished by hitherto known procedures. In particular, the finishing of a textile fabric with ethyl cellulose and a thermoplastic, alkali-resistant, synthetic resin compatible with ethyl cellulose makes it possible to provide fabrics having a substantially increased stiffness over that obtainable with ethyl cellulose and a plasticizer. Furthermore, the resin imparts to the finish an adhesive quality which contributes materially to retention of the finishing composition inthe fabric. The thermoplastic resin also lowers the fusing point of the ethyl cellulose composition in a manner far superior to its lowerin with plasticizers, and, moreover, prevents the rise in fusing point on successive launderings, the latter being a distinct disadvantage of fabrics finished with ethyl cellulose alone or ethyl cellulosecom-bined with a plasticizer. Compositions of ethyl cellulose alone or ethyl cellulose and a plasticizer show an undesirable rise in melting point on the fabric when the latter is washed and subsequently ironed. The fusing point of such compositions rapidly reach a point at which fusibility by ironing is either difllcult or requires an excessively high temperature. The permanency of the textile finish obtained by the process of this invention is a distinct improvement over those finishes which are lost on laundering, such as starch finishes. I

It will be understood that the details and examples hereinbefore set forth are illustrative only, and that the invention as herein broadly ods of preparation thereof? What I claim and desire to protect by Letters Patent is:

1. A permanently sized textile fabric characterized by pliability and perviousness to bothmoisture ,and air and by having the individual threads thereof impregnated with a solid thermomoplastic composition comprisin ethyl cellulose and a thermoplastic, alkali-resistant, polymerized hydrocarbon resin compatible with ethyl cellulose, said fabric being substantially resistant to the action of aqueous alkaline solutions and containing insufficient thermoplastic composition to fill the interstices or to form a continuous coating over the surface of the fabric.

3. A permanently sized textile fabric characterized by pliability and perviousness to both moisture and air and by havingthe individual threads thereof impregnated with a solid, thermoplastic composition comprising ethyl cellulose and a thermoplastic, alkali-resistant, hydrogenated polymerized hydrocarbon resin compatible with ethyl cellulose, said fabric being substantially resistant to the action of aqueous alkaline solutions and containing insufficient thermoplastic composition to fill the interstices or to form a continuous coating over the surface of the fabric.

4. A permanently sized textile fabric characterized by pliability and perviousness to both moisture and air and by having the individual threads thereof impregnated with a solid thermoplastic composition comprising ethyl cellulose and a thermoplastic, alkali-resistant, rosinmodified alkyd resin compatible with ethyl cellulose, said fabric being. substantially resistant to the action of aqueous alkaline solutions and containing insufficient thermoplastic composition to fill the interstices or to'form a continuous coatin over the surface of the fabric.

5. A permanently sized textile fabric characterized by pliability and perviousness to both moisture and air and by having the individual threads thereof impregnated with a solid thermoplastic composition comprising ethyl cellulose and a thermoplastic, alkali-resistant, rosin-modified maleate resin compatible withethyl cellulose, said fabric being substantially resistant to the action of aqueous alkaline solutions and containing insufiicient thermoplastic composition to fill the interstices or to form a continuous coating over the surface of the fabric. I

6. A permanently sized textile fabric characterized by pliability and perviousness to both moisture and air and by having the individual threads thereof impregnated with a solid thermoplastic composition comprising ethyl cellulose and a polyhydric alcohol ester of hydrogenated rosin, compatible with ethyl cellulose, said fabric being terized by pliability and perviousness to both moisture and air and by having the individual threads thereof impregnated with a solid thermoplastic composition comprising ethyl cellulose and 9, glycerol ester of hydrogenated rosin, said fabric being substantially resistant to the action of aqueous alkaline solutions and containing insufficient thermoplastic composition to fill the interstices or to form a. continuous coating over the surface of the fabric. v

8. A permanently sized textile fabric characterized by pliability and perviousness to both moisture and .air and by having the individual threads thereof impregnated with a solid thermoplastic composition comprising ethyl cellulose, a

plasticizer, and a thermoplastic, alkali-resistant, rosin-modified maleate resin compatible with ethyl cellulose, said fabric being substantially resistant to the action of aqueous alkaline solutions and containing insufficient thermoplastic composition to fill the interstices or to form a continuous coating over the surface of the fabric;

9. A permanently sized textile fabric characterized by pliability and perviousness to both moisture and air and by having the individual threads thereof impregnated with a solid thermoplastic composition comprising ethyl cellulose, a plasticizer, and a glycerol ester of hydrogenated rosin compatible with ethyl cellulose, said fabric being substantially resistant to the action of aqueous alkaline solutions and containing insufficient thermoplastic composition to fill the interstices or to form a continuous coating over the surface of the fabric. I

10. A method for the production of a permanently sized textile fabric characterized by pliability and perviousness to both moisture and air which includes impregnating a fabric with an aqueous emulsion of -a substantially water-immiscible solution of a solid thermoplastic composition comprising ethyl cellulose and a thermoplastic, alkali-resistant, synthetic resin compatible with ethyl cellulose, removing the excess emulsion from the fabric, evaporating the waterand volatilesolvent from the emulsion contained in the said fabric, and then pressing the fabric at an elevated temperature.

11. A method for'the production of apermanently sized textile fabric characterized by pliability and perviousness to both moisture and air which includes impregnating a fabric with an aqueous emulsion of a substantially water-immiscible solution of a solid thermoplastic composition'comprising ethyl cellulose and a thermoplastic, alkaliresistant, polymerized hydrocarbon resin compatible with ethyl cellulose, removing the excess emulsion from the fabric, evaporating the water and volatile solvent from the emulsion contained in the said fabric, and then pressing the fabric at an. elevated temperature,

' 12. A method for the production of a permawithin the range of about 180 F. to about 400 F.

nently sized textile fabric characterized by plicible solution of a solid thermoplastic composition comprising ethyl cellulose and a thermoplastic, alkali-resistant, rosin-modified alkyd resin bility and perviousness to both moisture and air which includes impregnating a fabric with an aqueous emulsion of a substantially water-immiscible solution of a solid thermoplastic composition comprising ethyl cellulose and a polyhydric alcohol ester of hydrogenated rosin, removing the excess emulsion from the fabric, evaporating the water and volatile solvent from the emulsion contained in the said fabric, and then pressing the fabric at an elevated temperature.

14. A method for the production of a permanently sized textile fabric characterized by pliability and perviousness to both moisture and air which includes impregnating a fabric with an aqueous emulsion of a substantially water-immiscible solutionof a solid thermoplastic composition comprising ethyl cellulose and a thermoplastic, alkali-resistant, synthetic resin compatible with ethyl cellulose, removing the excess emulsion from the fabric so that the emulsion remaining therein will, on drying, leave no more than about 40% by weight of non-volatile material in the fabric based on the weight of the fabric, evaporatin'g the water and volatile solvent from the emulsion contained in the said fabric, and then pressing the fabric at an elevated temperature.

15. A method for the production of a permanently sized textile fabric characterized by pliacible solution of a solid thermoplastic composition comprising ethyl cellulose and a thermoplastic, alkali-resistant, synthetic resin compatible with ethyl cellulose, removing the excess emulsion from the fabric so that the emulsion remaining therein will, on drying, leave no more than about 40% by weight of non-volatile material in the fabric based on the weight of "the fabric, evaporating the water and volatile solvent from the emulsion contained in the said fabric, and then pressing the fabric at a temperature 16. A method for the production of a permanently sized textile fabric characterized by pliability and perviousness to both moisture and air which includes impregnating a fabric with an aqueous emulsion of a substantially water-immiscible solution of a solid thermoplastic composition comprising ethyl cellulose and a thermoplastic, alkali-resistant, synthetic resin compatible with ethyl cellulose, removing the excess emulsion from the fabric so that the emulsion remaining therein will, on drying, leave no more than about 40% by weight of non-volatile material in the fabric based on the weight of the fabric,- evaporating the water and volatile solvent from the emulsion contained in the said fabric.

and then pressing the fabric at a temperature within the range of about 240 F. to about 280 I".

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